# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chris Russell' _publ_contact_author_address ; Dr. Chris Russell School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287599' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email Chris.Russell@bristol.ac.uk _publ_section_title ; Cationic phosphorus/carbon/pnictogen cages isolobal to [C5R5]+ ; loop_ _publ_author_name 'C. Russell' 'Cheryl Fish' 'Michael Green' 'John C. Jeffery' 'Richard J. Kilby' 'Jason Martin Lynam' ; J.McGrady ; 'Dimitrios Pantazis' 'Charlotte E. Willans' data_3+AlCl4- _database_code_depnum_ccdc_archive 'CCDC 293301' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C10 H18 Al Cl4 P2 Sb' _chemical_formula_weight 490.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.1431(4) _cell_length_b 9.8320(5) _cell_length_c 11.0710(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.6970(10) _cell_angle_gamma 90.00 _cell_volume 918.15(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5620 _cell_measurement_theta_min 4.829 _cell_measurement_theta_max 54.901 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method none _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 2.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.192 _diffrn_detector_type 'Bruker-AXS SMART 1k' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation '0.5 mm double pin hole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9862 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2224 _reflns_number_gt 1981 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.6939P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2224 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.32791(3) 0.2500 0.80991(2) 0.04297(10) Uani 1 2 d S . . P1 P 0.10368(8) 0.11138(6) 0.64631(6) 0.02885(14) Uani 1 1 d . . . C1 C 0.0497(3) 0.2500 0.7275(3) 0.0209(6) Uani 1 2 d S . . C6 C 0.1826(3) 0.2500 0.5831(3) 0.0203(6) Uani 1 2 d S . . C2 C -0.0418(4) 0.2500 0.8160(3) 0.0241(6) Uani 1 2 d S . . C3 C -0.0052(5) 0.1231(4) 0.8994(4) 0.0740(13) Uani 1 1 d . . . H3A H 0.1074 0.1225 0.9571 0.111 Uiso 1 1 calc R . . H3B H -0.0293 0.0427 0.8427 0.111 Uiso 1 1 calc R . . H3C H -0.0698 0.1219 0.9524 0.111 Uiso 1 1 calc R . . C4 C -0.2185(5) 0.2500 0.7300(4) 0.0600(13) Uani 1 2 d S . . H4A H -0.2408 0.1789 0.6632 0.090 Uiso 0.50 1 calc PR . . H4B H -0.2485 0.3388 0.6873 0.090 Uiso 0.50 1 calc PR . . H4C H -0.2795 0.2323 0.7842 0.090 Uiso 0.50 1 calc PR . . C7 C 0.2591(3) 0.2500 0.4844(3) 0.0212(6) Uani 1 2 d S . . C8 C 0.3606(3) 0.1216(2) 0.4999(3) 0.0325(5) Uani 1 1 d . . . H8A H 0.4476 0.1220 0.5863 0.049 Uiso 1 1 calc R . . H8B H 0.4042 0.1201 0.4318 0.049 Uiso 1 1 calc R . . H8C H 0.2947 0.0407 0.4916 0.049 Uiso 1 1 calc R . . C9 C 0.1253(4) 0.2500 0.3469(3) 0.0315(7) Uani 1 2 d S . . H9A H 0.0688 0.1630 0.3318 0.047 Uiso 0.50 1 calc PR . . H9B H 0.1709 0.2628 0.2808 0.047 Uiso 0.50 1 calc PR . . H9C H 0.0512 0.3242 0.3406 0.047 Uiso 0.50 1 calc PR . . Al1 Al 0.58816(11) 0.2500 0.19853(9) 0.0251(2) Uani 1 2 d S . . Cl1 Cl 0.73999(10) 0.2500 0.40071(8) 0.03146(18) Uani 1 2 d S . . Cl2 Cl 0.72218(12) 0.2500 0.07853(10) 0.0537(3) Uani 1 2 d S . . Cl3 Cl 0.43933(8) 0.07381(7) 0.15331(7) 0.04500(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.01961(13) 0.0838(2) 0.02243(14) 0.000 0.00471(9) 0.000 P1 0.0397(3) 0.0196(3) 0.0373(3) -0.0017(2) 0.0260(3) -0.0029(2) C1 0.0179(13) 0.0228(13) 0.0217(14) 0.000 0.0074(11) 0.000 C6 0.0184(13) 0.0227(14) 0.0195(14) 0.000 0.0069(11) 0.000 C2 0.0243(15) 0.0315(16) 0.0188(14) 0.000 0.0108(12) 0.000 C3 0.095(3) 0.078(2) 0.082(3) 0.046(2) 0.071(2) 0.039(2) C4 0.034(2) 0.112(4) 0.040(2) 0.000 0.0211(19) 0.000 C7 0.0205(14) 0.0220(14) 0.0245(15) 0.000 0.0124(12) 0.000 C8 0.0345(12) 0.0296(11) 0.0415(14) 0.0021(10) 0.0238(11) 0.0079(10) C9 0.0308(17) 0.0393(18) 0.0272(17) 0.000 0.0144(14) 0.000 Al1 0.0230(5) 0.0324(5) 0.0188(4) 0.000 0.0070(4) 0.000 Cl1 0.0312(4) 0.0386(4) 0.0202(4) 0.000 0.0051(3) 0.000 Cl2 0.0393(5) 0.0974(9) 0.0311(5) 0.000 0.0210(4) 0.000 Cl3 0.0386(3) 0.0394(3) 0.0483(4) -0.0075(3) 0.0071(3) -0.0097(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C6 2.344(3) . ? Sb1 C1 2.348(3) . ? Sb1 P1 2.5447(7) . ? Sb1 P1 2.5447(7) 4_565 ? P1 C1 1.803(2) . ? P1 C6 1.805(2) . ? C1 C2 1.515(4) . ? C1 P1 1.803(2) 4_565 ? C6 C7 1.508(4) . ? C6 P1 1.805(2) 4_565 ? C2 C3 1.510(4) 4_565 ? C2 C3 1.510(4) . ? C2 C4 1.526(5) . ? C7 C8 1.537(3) 4_565 ? C7 C8 1.537(3) . ? C7 C9 1.542(4) . ? Al1 Cl2 2.1267(13) . ? Al1 Cl1 2.1306(12) . ? Al1 Cl3 2.1395(8) . ? Al1 Cl3 2.1395(8) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Sb1 C1 60.17(10) . . ? C6 Sb1 P1 43.09(5) . . ? C1 Sb1 P1 43.02(5) . . ? C6 Sb1 P1 43.09(5) . 4_565 ? C1 Sb1 P1 43.02(5) . 4_565 ? P1 Sb1 P1 64.77(3) . 4_565 ? C1 P1 C6 81.36(10) . . ? C1 P1 Sb1 62.66(9) . . ? C6 P1 Sb1 62.52(9) . . ? C2 C1 P1 130.42(8) . . ? C2 C1 P1 130.42(8) . 4_565 ? P1 C1 P1 98.20(15) . 4_565 ? C2 C1 Sb1 122.3(2) . . ? P1 C1 Sb1 74.32(9) . . ? P1 C1 Sb1 74.32(9) 4_565 . ? C7 C6 P1 130.37(8) . . ? C7 C6 P1 130.37(8) . 4_565 ? P1 C6 P1 98.07(14) . 4_565 ? C7 C6 Sb1 123.2(2) . . ? P1 C6 Sb1 74.39(10) . . ? P1 C6 Sb1 74.39(10) 4_565 . ? C3 C2 C3 111.3(4) 4_565 . ? C3 C2 C1 110.34(19) 4_565 . ? C3 C2 C1 110.34(19) . . ? C3 C2 C4 108.3(2) 4_565 . ? C3 C2 C4 108.3(2) . . ? C1 C2 C4 108.2(3) . . ? C6 C7 C8 110.35(17) . 4_565 ? C6 C7 C8 110.35(17) . . ? C8 C7 C8 110.5(3) 4_565 . ? C6 C7 C9 107.6(2) . . ? C8 C7 C9 108.99(18) 4_565 . ? C8 C7 C9 108.99(18) . . ? Cl2 Al1 Cl1 110.94(6) . . ? Cl2 Al1 Cl3 108.76(4) . . ? Cl1 Al1 Cl3 110.10(4) . . ? Cl2 Al1 Cl3 108.76(4) . 4_565 ? Cl1 Al1 Cl3 110.09(4) . 4_565 ? Cl3 Al1 Cl3 108.13(6) . 4_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.743 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.076 #===END data_2+AlCl4- _database_code_depnum_ccdc_archive 'CCDC 293302' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C10 H18 Al As Cl4 P2' _chemical_formula_weight 443.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.1632(8) _cell_length_b 9.6826(4) _cell_length_c 20.9520(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.2530(10) _cell_angle_gamma 90.00 _cell_volume 3812.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6342 _cell_measurement_theta_min 4.732 _cell_measurement_theta_max 54.412 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method none _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 173 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.192 _diffrn_detector_type 'Bruker-AXS SMART 1k' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Platform' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation '0.5 mm double pin hole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_target Mo _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19900 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4359 _reflns_number_gt 3411 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+1.7207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4359 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.090491(14) 0.50695(3) 0.151373(13) 0.03004(8) Uani 1 1 d . . . P1 P 0.11062(4) 0.56377(7) 0.04703(3) 0.02997(15) Uani 1 1 d . . . C1 C 0.18446(12) 0.5123(2) 0.11021(11) 0.0247(5) Uani 1 1 d . . . P2 P 0.18829(3) 0.66002(7) 0.16265(3) 0.02871(15) Uani 1 1 d . . . C6 C 0.10713(12) 0.6989(2) 0.10582(11) 0.0244(5) Uani 1 1 d . . . C2 C 0.23481(13) 0.3908(2) 0.11301(12) 0.0285(5) Uani 1 1 d . . . C3 C 0.19342(17) 0.2611(3) 0.08669(18) 0.0548(9) Uani 1 1 d . . . H3A H 0.1587 0.2390 0.1138 0.082 Uiso 1 1 calc R . . H3B H 0.2265 0.1837 0.0875 0.082 Uiso 1 1 calc R . . H3C H 0.1686 0.2775 0.0418 0.082 Uiso 1 1 calc R . . C4 C 0.27355(16) 0.3665(3) 0.18289(14) 0.0445(7) Uani 1 1 d . . . H4A H 0.3004 0.4495 0.1993 0.067 Uiso 1 1 calc R . . H4B H 0.3064 0.2885 0.1841 0.067 Uiso 1 1 calc R . . H4C H 0.2388 0.3458 0.2102 0.067 Uiso 1 1 calc R . . C5 C 0.28953(16) 0.4287(3) 0.07123(16) 0.0509(8) Uani 1 1 d . . . H5A H 0.2649 0.4470 0.0265 0.076 Uiso 1 1 calc R . . H5B H 0.3229 0.3519 0.0714 0.076 Uiso 1 1 calc R . . H5C H 0.3157 0.5114 0.0891 0.076 Uiso 1 1 calc R . . C7 C 0.05824(13) 0.8222(2) 0.10374(13) 0.0311(6) Uani 1 1 d . . . C8 C -0.01541(13) 0.7895(3) 0.06324(14) 0.0379(6) Uani 1 1 d . . . H8A H -0.0107 0.7625 0.0192 0.057 Uiso 1 1 calc R . . H8B H -0.0458 0.8714 0.0610 0.057 Uiso 1 1 calc R . . H8C H -0.0368 0.7135 0.0836 0.057 Uiso 1 1 calc R . . C9 C 0.05164(17) 0.8637(3) 0.17298(14) 0.0499(8) Uani 1 1 d . . . H9A H 0.0302 0.7877 0.1933 0.075 Uiso 1 1 calc R . . H9B H 0.0215 0.9460 0.1712 0.075 Uiso 1 1 calc R . . H9C H 0.0990 0.8840 0.1987 0.075 Uiso 1 1 calc R . . C10 C 0.09220(16) 0.9388(3) 0.07034(17) 0.0486(8) Uani 1 1 d . . . H10A H 0.1393 0.9605 0.0961 0.073 Uiso 1 1 calc R . . H10B H 0.0620 1.0212 0.0670 0.073 Uiso 1 1 calc R . . H10C H 0.0969 0.9091 0.0267 0.073 Uiso 1 1 calc R . . Al1 Al 0.88749(4) 0.33519(8) 0.15146(4) 0.02782(17) Uani 1 1 d . . . Cl1 Cl 0.87836(4) 0.21860(7) 0.23554(3) 0.04216(17) Uani 1 1 d . . . Cl2 Cl 0.78901(4) 0.33720(9) 0.08270(4) 0.0517(2) Uani 1 1 d . . . Cl3 Cl 0.96694(4) 0.24561(7) 0.10596(3) 0.04210(17) Uani 1 1 d . . . Cl4 Cl 0.91521(4) 0.54330(7) 0.17980(4) 0.04469(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.02706(14) 0.02876(14) 0.03661(16) 0.00716(11) 0.01198(11) -0.00063(11) P1 0.0329(4) 0.0310(3) 0.0244(4) -0.0007(3) 0.0015(3) 0.0036(3) C1 0.0241(12) 0.0246(12) 0.0261(13) 0.0012(9) 0.0069(10) -0.0030(10) P2 0.0250(3) 0.0275(3) 0.0320(4) -0.0051(3) 0.0015(3) 0.0001(3) C6 0.0230(12) 0.0233(12) 0.0277(13) 0.0027(9) 0.0065(10) -0.0028(9) C2 0.0271(13) 0.0253(12) 0.0346(15) 0.0011(10) 0.0099(11) 0.0021(10) C3 0.0479(19) 0.0297(15) 0.084(3) -0.0183(15) 0.0059(17) 0.0043(13) C4 0.0452(17) 0.0439(16) 0.0427(18) 0.0075(13) 0.0041(14) 0.0168(13) C5 0.0482(19) 0.0529(19) 0.060(2) 0.0119(16) 0.0319(16) 0.0190(15) C7 0.0327(14) 0.0256(12) 0.0360(15) 0.0033(10) 0.0095(12) 0.0042(11) C8 0.0285(14) 0.0445(15) 0.0415(17) 0.0104(13) 0.0088(12) 0.0069(12) C9 0.056(2) 0.0459(17) 0.0465(19) -0.0103(14) 0.0073(15) 0.0181(15) C10 0.0398(17) 0.0288(14) 0.078(2) 0.0129(15) 0.0151(16) 0.0037(13) Al1 0.0269(4) 0.0298(4) 0.0272(4) 0.0010(3) 0.0064(3) -0.0032(3) Cl1 0.0483(4) 0.0451(4) 0.0333(4) 0.0085(3) 0.0088(3) -0.0068(3) Cl2 0.0348(4) 0.0671(5) 0.0477(5) 0.0178(4) -0.0056(3) -0.0077(4) Cl3 0.0442(4) 0.0438(4) 0.0416(4) -0.0059(3) 0.0164(3) 0.0062(3) Cl4 0.0528(4) 0.0311(3) 0.0560(5) -0.0070(3) 0.0252(4) -0.0077(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C6 2.141(2) . ? As1 C1 2.144(2) . ? As1 P1 2.3581(7) . ? As1 P2 2.3648(7) . ? P1 C6 1.807(2) . ? P1 C1 1.809(2) . ? C1 C2 1.516(3) . ? C1 P2 1.796(2) . ? P2 C6 1.804(2) . ? C6 C7 1.514(3) . ? C2 C4 1.525(4) . ? C2 C3 1.530(4) . ? C2 C5 1.536(4) . ? C7 C8 1.532(4) . ? C7 C9 1.534(4) . ? C7 C10 1.538(4) . ? Al1 Cl1 2.1280(10) . ? Al1 Cl3 2.1320(10) . ? Al1 Cl4 2.1383(10) . ? Al1 Cl2 2.1392(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 As1 C1 65.78(9) . . ? C6 As1 P1 47.05(7) . . ? C1 As1 P1 47.09(7) . . ? C6 As1 P2 46.88(6) . . ? C1 As1 P2 46.64(6) . . ? P1 As1 P2 71.13(2) . . ? C6 P1 C1 80.10(11) . . ? C6 P1 As1 60.15(7) . . ? C1 P1 As1 60.22(7) . . ? C2 C1 P2 130.15(18) . . ? C2 C1 P1 130.04(18) . . ? P2 C1 P1 99.27(11) . . ? C2 C1 As1 122.96(16) . . ? P2 C1 As1 73.17(8) . . ? P1 C1 As1 72.69(8) . . ? C1 P2 C6 80.52(11) . . ? C1 P2 As1 60.19(7) . . ? C6 P2 As1 60.03(7) . . ? C7 C6 P2 129.24(18) . . ? C7 C6 P1 131.05(18) . . ? P2 C6 P1 99.05(11) . . ? C7 C6 As1 123.55(16) . . ? P2 C6 As1 73.09(8) . . ? P1 C6 As1 72.80(8) . . ? C1 C2 C4 110.1(2) . . ? C1 C2 C3 110.0(2) . . ? C4 C2 C3 109.9(2) . . ? C1 C2 C5 107.0(2) . . ? C4 C2 C5 109.0(2) . . ? C3 C2 C5 110.8(2) . . ? C6 C7 C8 110.5(2) . . ? C6 C7 C9 110.1(2) . . ? C8 C7 C9 109.9(2) . . ? C6 C7 C10 106.1(2) . . ? C8 C7 C10 109.0(2) . . ? C9 C7 C10 111.0(2) . . ? Cl1 Al1 Cl3 109.61(4) . . ? Cl1 Al1 Cl4 109.03(4) . . ? Cl3 Al1 Cl4 110.32(4) . . ? Cl1 Al1 Cl2 110.98(4) . . ? Cl3 Al1 Cl2 108.40(4) . . ? Cl4 Al1 Cl2 108.49(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.393 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.070